Granular detergent component and process for its preparation

ABSTRACT

A granular detergent component comprising a high level of surfactant, for example, cationic surfactant, and an inorganic carrier material is prepared by a process involving spraying an aqueous solution of the surfactant onto moving granules of the inorganic carrier material in the presence of a drying gas, preferably air, at a temperature within the range of from 65 to 200° C. The process is preferably carried out in a fluidised bed. Preferred inorganic carrier materials are sodium carbonate and zeolite MAP.

TECHNICAL FIELD

[0001] The present invention relates to a granular detergent componentsuitable for incorporation into particulate laundry detergentcompositions, and a novel process for its preparation. The granulardetergent component contains a cationic, zwitterionic or amphotericsurfactant.

BACKGROUND

[0002] Cationic, amphoteric and zwitterionic surfactants are usefulingredients in laundry detergent compositions, generally used inrelatively minor amounts as co-surfactants to supplement non-soapanionic surfactants and, in some cases, nonionic surfactants.

[0003] These materials are commercially available as aqueous solutionsof relatively low concentration, generally below 50 wt %, for example,30 to 40 wt %. For some materials, for example, water-soluble quaternaryammonium cationic surfactants having a single long hydrocarbon chain,mobile solutions of higher concentration are not possible becausegelling occurs.

[0004] While these solutions may be suitable for inclusion in liquiddetergent compositions, or for incorporation in detergent powders viatraditional slurry-making and spray-drying processes, the large amountof associated water can pose problems in preparing granular detergentcompositions or components by non-spray-drying (mixing and granulation)processes. For incorporation into “compact” or “concentrated” laundrypowders, a granule containing a relatively high surfactant loading isrequired.

PRIOR ART

[0005] WO 96 17042A (Procter & Gamble) discloses detergent granulescontaining a water-soluble cationic surfactant and an inorganic carrier,the granules also containing an anionic surfactant in a weight ratio tothe cationic surfactant of less than 1:1, and preferably less than0.5:1. The inorganic carrier material is zeolite. The granules areprepared by evaporating and concentrating a solution of the cationic andanionic surfactants to a concentration above 50 wt %, and thengranulating with the carrier material. The presence of the anionicsurfactant prevents gelling during the concentration step.

[0006] WO 98/53037A (Procter & Gamble) discloses a process for thepreparation of cationic surfactant granules, in which a aqueous solutionor dispersion of cationic surfactant, optionally plus sodium silicateand/or filler, is dried in the presence of a drying gas, preferably air,at a temperature of less than 250° C. The preferred drying method isco-current spray-drying.

[0007] The present inventors have now discovered that granulescontaining more than 20 wt % of cationic, amphoteric or zwitterionicsurfactant may be obtained in a non-spray-drying process, without theneed for elevated temperatures and without the need for anionicsurfactant.

DEFINITION OF THE INVENTION

[0008] The invention accordingly provides a process for the preparationof a granular detergent component comprising

[0009] (a) at least 20 wt % of a surfactant selected from cationicsurfactants, zwitterionic surfactants, amphoteric surfactants andmixtures thereof,

[0010] (b) an inorganic carrier material,

[0011] which process comprises spraying an aqueous solution of thesurfactant (a) onto moving granules of the inorganic carrier material(b) in the presence of a drying gas at a temperature within the range offrom 65 to 200° C., preferably from 80 to 200° C., and more preferablyfrom 100 to 150° C.

[0012] In a second aspect, the present invention provides a granulardetergent component comprising

[0013] (a) at least 20 wt % of a surfactant selected from cationicsurfactants, zwitterionic surfactants, amphoteric surfactants andmixtures thereof,

[0014] (b) an inorganic carrier material,

[0015] the granular detergent component being free of sodium sulphate.

[0016] In a third aspect, the present invention provides a particulatelaundry detergent composition comprising in total from 5 to 60 wt % ofone or more organic detergent surfactants, from 10 to 80 wt % of one ormore detergency builders and optionally other detergent ingredients,which composition includes a granular detergent component as definedabove.

DETAILED DESCRIPTION OF THE INVENTION The Cationic, Amphoteric orZwitterionic Surfactant

[0017] The invention is applicable to any cationic, amphoteric orzwitterionic surfactant which is supplied as a relatively dilute (forexample, less than 50 wt %) aqueous solution. It is especiallyapplicable to such surfactants which are sensitive to heat and liable todegradation or decomposition at temperatures above 200° C., or evenabove 150° C.

[0018] Preferred water-soluble cationic surfactants are quaternaryammonium salts of the general formula I

R₁R₂R₃R₄N⁺X⁻  (I)

[0019] wherein R₁ is a relatively long (C₈-C₁₈) hydrocarbon chain,typically an alkyl, hydroxyalkyl or ethoxylated alkyl group, optionallyinterrupted with a heteroatom or an ester or amide group; each of R₂, R₃and R₄ (which may be the same or different) is a short-chain (C₁-C₃)alkyl or substituted alkyl group; and X is a solubilising anion, forexample a chloride, bromide or methosulphate ion.

[0020] In a preferred class of compounds, R₁ is a C₈-C₁₈ alkyl group,more preferably a C₈-C₁₀ or C₁₂-C₁₄ alkyl group, R₂ is a methyl group,and R₃ and R₄, which may be the same or different, are methyl orhydroxyethyl groups.

[0021] In an especially preferred compound, R₁ is a C₁₂-C₁₄ alkyl group,R₂ and R₃ are methyl groups, R₄ is a 2-hydroxyethyl group, and X⁻ is achloride ion. This material is available commercially as Praepagen(Trade Mark) HY from Clariant GmbH, in the form of a 40 wt % aqueoussolution.

[0022] Other classes of cationic surfactant include cationic esters (forexample, choline esters).

[0023] Preferred zwitterionic surfactants include betaines of theformula II

[0024] wherein R₅ is a hydrocarbon chain containing 8 to 20 carbonatoms, optionally interrupted by an amide group, and m is an integerfrom 1 to 4.

[0025] Especially preferred zwitterionic surfactants are betaines of theformula IIa

[0026] wherein R₆ is a C₈-C₁₈ alkyl group, and n is an integer of from 2to 4.

[0027] An especially preferred material is cocoamidopropyl betaine(CAPB), in which R₆ is C₁₂-C₁₄ alkyl and m is 3.

[0028] Preferred amphoteric surfactants include alkyl amine oxides ofthe general formula III

R₇R₈R₉N→O  (III)

[0029] wherein R₇ is typically a C₈-C₁₈ alkyl group, for example,C₁₂-C₁₄ alkyl, and R₈ and R₉, which may be the same or different, areC₁-C₃ alkyl or hydroxyalkyl groups, for example, methyl groups. The mostpreferred amine oxide is coco dimethylamine oxide, in which R₇ isC₁₂-C₁₄ alkyl and R₈ and R₉ are methyl groups.

The Inorganic Carrier Material

[0030] The granular detergent component of the invention contains, as anessential ingredient, an inorganic carrier material.

[0031] According to a first preferred embodiment of the invention, theinorganic carrier material consists to an extent of at least 80 wt % ofwater-soluble material. The use of a predominantly water soluble carriermaterial is believed to be particularly advantageous in productsintended for laundering by hand.

[0032] Preferred water-soluble carrier materials are sodium carbonate,sodium tripolyphosphate and mixtures thereof. Sodium carbonate isespecially preferred.

[0033] In this embodiment of the invention, up to 20 wt % of theinorganic carrier material may be constituted by water-insolublematerial. Preferred water-insoluble carrier materials arealuminosilicates, particularly crystalline alkali metal aluminosilicates(zeolites), silicas, calcites and clays.

[0034] Thus, advantageously the inorganic carrier material comprisesfrom 80 to 100 wt % of sodium carbonate, and optionally up to 20 wt % ofwater-insoluble carrier material selected from crystalline alkali metalaluminosilicates (zeolites), silicas, calcites and clays.

[0035] In a second preferred embodiment of the invention, the inorganiccarrier consists at least partially of water-insoluble material.Preferably the inorganic carrier material comprises from 80 to 100 wt %of water insoluble material. Advantageously, the inorganic carriermaterial may comprise from 20 to 100 wt % of crystalline alkali metalaluminosilicate. Most preferably, the inorganic carrier materialcomprises from 80 to 100 wt % of crystalline alkali metalaluminosilicate.

[0036] Preferred water-insoluble carrier materials are aluminosilicates,silicas, clays, calcite and mixtures thereof. Crystalline alkali metalaluminosilicate (zeolite) is preferred. An especially preferred zeolitematerial is zeolite MAP, commercially available from Crosfield Chemicalsas Doucil (Trade Mark) A24. An alternative zeolite material is zeolite Apowder, available, for example, as Wessalith (Trade Mark) P from DegussaAG.

[0037] The choice of carrier material may be dictated by the detergentformulation into which the granular component is to be incorporated. Theprocess of the invention is sufficiently flexible to accommodate anyinorganic granular material having sufficient carrying capacity.

The Process

[0038] As previously indicated, the granular detergent component isprepared by a non-spray-drying process in which an aqueous solution ofthe surfactant (a) is sprayed onto moving granules of the inorganiccarrier material (b) in the presence of a drying gas at a temperature offrom 65 to 200° C., preferably 80 to 200° C., more preferably from 100to 150° C.

[0039] In the process of the invention, as the surfactant solutioncontacts the carrier granules, water is simultaneously rapidly drivenoff. The formation of gel phases of intermediate concentration is thusavoided and it is unnecessary to include special ingredients such asanionic surfactants in order to avoid gelling. This is achieved withoutthe necessity for high temperatures, for example above 250° C., whichcould cause degradation of the surfactant (a). The process of theinvention thus enables the large amount of water associated with thesurfactant (a) in the starting solution to be driven off, as thesolution encounters the granules of carrier material, without theformation of unprocessable gel phases, and without the use of hightemperatures which could cause decomposition or degradation of thesurfactant (a).

[0040] The maximum temperature during the process is no higher than 200°C. and is preferably no higher than 150° C.

[0041] The starting surfactant solution preferably has a concentrationof less than 50 wt %, and preferably within the range of from 30 to 45wt %. The upper limit will depend on the particular surfactant and theconcentration at which the solution becomes too viscous for spraying.The lower limit is a matter of practicality because if the amount ofwater is too high the process will be too slow and consume too muchenergy to be economic.

[0042] According to a preferred embodiment of the invention, the processis carried out in a fluidised bed. This preferred process of theinvention comprises the steps of:

[0043] (i) fluidising granules of the inorganic carrier material (b)using a gas having a temperature within the range of from 100 to 150°C.,

[0044] (ii) spraying an aqueous solution of the surfactant (a) onto themass of fluidised granules,

[0045] (iii) cooling the resulting granular detergent component bymixing in the presence of a gas having a temperature not exceeding 50°C.

[0046] Preferably, the drying and cooling gases used in steps (i) and(iii) are air. The preferred cooling gas is air at ambient temperature.

[0047] The aqueous solution of the surfactant (a) is advantageouslypreheated to a temperature within the range of from 50 to 70° C.

[0048] In this embodiment, granules of carrier material are fluidisedusing a drying gas, preferably air, for example, at 100 to 150° C.Surfactant solution, preferably preheated to 50 to 70° C., is sprayedonto the mass of fluidised granules. After sufficient surfactantsolution has been added to attain the desired concentration in the finalproduct, for example, 20 to 40 wt %, the granules are cooled.

[0049] The cooling step (iii) is preferably carried out in a fluidisedbed. The heating (spraying-on) and cooling stages of the process may becarried out within a single fluidised bed, either operating in alternateheating and cooling cycles, or divided into two sections, one for theheating stage and the other for the cooling stage. Alternatively, twofluid beds in series may be used.

[0050] The use of a fluidised bed for heating (spraying-on) step solvesthe problem of driving off the water from the surfactant solutionsufficiently rapidly to avoid the formation of higher-concentration gelphases, while avoiding temperatures that would cause decomposition ordegradation of the surfactant.

[0051] According to an alternative embodiment of the invention, theprocess may be carried out in a flash dryer, either under vacuum or atatmospheric pressure.

[0052] The granules may subsequently be layered with a finely dividedflow aid in any suitable mixer. Preferred flow aids are selected fromzeolites and amorphous aluminosilicates.

[0053] In a preferred embodiment the process is carried out as a batchprocess.

[0054] The process may advantageously include a preliminary step whereina partial quantity of the surfactant is added to the inorganic carriermaterial prior to the main process step or steps.

[0055] This may be of particular value when the carrier material iszeolite, more particularly zeolite MAP which typically has an averageprimary particle size of 0.1-5 micrometres.

[0056] The preliminary step is suitably carried out in amixer/granulator. Alternatively it may be carried out in a fluidised bedhaving a substantially reduced gas flow rate than used in the mainprocess.

[0057] Including the preliminary step improves the process by allowing ahigher initial gas velocity in the main fluidised bed process due to theincreased size of the constituent particles of the inorganic carriermaterial, thus reducing batch times, or increasing throughput in acontinuous process. The preliminary step may also be beneficial inenabling greater levels of the surfactant to be added to the inorganiccarrier material, whether or not the carrier material has a smallparticle size.

The Granular Detergent Component

[0058] The granular detergent component of the invention contains, asessential ingredients, the surfactant (a) and the inorganic carriermaterial (b).

[0059] The component contains at least 20 wt % of the surfactant (a),and preferably contains at least 30 wt %. Typically the component willcontain from 20 to 40 wt % of the surfactant (a), more preferably from25 to 35 wt %.

[0060] The inorganic carrier material is preferably present in a totalamount of from 50 to 80 wt %, more preferably from 60 to 75 wt %.

[0061] Advantageously, the granular component may have an outer layer orcoating of finely divided water-insoluble flow aid, preferably selectedfrom zeolites and amorphous aluminosilicates. The flow aid is preferablypresent in an amount of from 1 to 5 wt %, more preferably from 1 to 3 wt%. The most preferred flow aid is zeolite powder.

[0062] In the first preferred embodiment of the invention, the granularcomponent may suitably comprise:

[0063] from 20 to 40 wt %, preferably from 25 to 35 wt %, of thesurfactant (a),

[0064] from 60 to 75 wt %, preferably from 65 to 70 wt %, of sodiumcarbonate,

[0065] from 1 to 5 wt %, preferably from 1 to 3 wt %, of zeolite, thezeolite being present as an outer layer or coating.

[0066] In the second preferred embodiment of the invention, the granularcomponent may suitably comprise:

[0067] from 20 to 40 wt %, preferably from 25 to 35 wt %, of thesurfactant (a),

[0068] from 60 to 80 wt %, preferably from 65 to 75 wt %, of zeolite.(zeolite may in part be present as coating)

[0069] If desired the granular component may contain a minor amount ofsodium silicate, but preferably the amount of silicate present is lessthan 5 wt %.

[0070] The granular component is preferably free of sodium sulphatewhich, although highly water-soluble, has insufficient carrying capacityto be useful.

[0071] Minor amounts of other materials may be present if desired, butthe granular component of the invention preferably does not containanionic surfactants.

Detergent Compositions

[0072] The granular detergent component of the invention provides aconvenient route for the incorporation into particulate detergentcompositions of surfactants which are available only as dilute aqueoussolutions. The granules may simply be dry-mixed with other particulateingredients or components to form the final detergent composition.

[0073] Accordingly, a further aspect of the invention provides aparticulate laundry detergent composition comprising in total from 5 to60 wt % of one or more organic detergent surfactants, from 10 to 80 wt %of one or more detergency builders and optionally other detergentingredients, which composition includes a granular detergent componentas defined above. Detergent compositions of the invention containdetergent-active compounds and detergency builders, and may optionallycontain bleaching components and other active ingredients to enhanceperformance and properties.

[0074] Detergent-active compounds (surfactants) may be chosen from soapand non-soap anionic, cationic, nonionic, amphoteric and zwitterionicdetergent-active compounds, and mixtures thereof. Many suitabledetergent-active compounds are available and are fully described in theliterature, for example, in “Surface-Active Agents and Detergents”,Volumes I and II, by Schwartz, Perry and Berch. The preferreddetergent-active compounds that can be used are soaps and syntheticnon-soap anionic and nonionic compounds. The total amount of surfactantpresent is suitably within the range of from 5 to 40 wt %.

[0075] Anionic surfactants are well-known to those skilled in the art.Examples include alkylbenzene sulphonates, particularly linearalkylbenzene sulphonates having an alkyl chain length of C₈-C₁₅; primaryand secondary alkylsulphates, particularly C₈-C₂₀ primary alkylsulphates; alkyl ether sulphates; olefin sulphonates; alkyl xylenesulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates.Sodium salts are generally preferred.

[0076] Nonionic surfactants that may be used include the primary andsecondary alcohol ethoxylates, especially the C₈-C₂₀ aliphatic alcoholsethoxylated with an average of from 1 to 20 moles of ethylene oxide permole of alcohol, and more especially the C₁₀-C₁₅ primary and secondaryaliphatic alcohols ethoxylated with an average of from 1 to 10 moles ofethylene oxide per mole of alcohol. Non-ethoxylated nonionic surfactantsinclude alkylpolyglycosides, glycerol monoethers, and polyhydroxyamides(glucamide).

[0077] The cationic, amphoteric and zwitterionic surfactants with whichthe present invention is concerned also form part of the surfactantsystem. They will generally be present in combination with anionicsurfactants, the weight ratio of anionic surfactant to cationic,amphoteric or zwitterionic surfactant being at least 1:1.

[0078] These lists of surfactants is not intended to be exhaustive andthe use of any surfactant suitable for incorporation in particulatelaundry detergent compositions falls within the scope of the presentinvention.

[0079] The detergent compositions of the invention also contain one ormore detergency builders. The total amount of detergency builder in thecompositions will suitably range from 5 to 80 wt %, preferably from 10to 60 wt %.

[0080] Preferred builders are alkali metal aluminosilicates, moreespecially crystalline alkali metal aluminosilicates (zeolites),preferably in sodium salt form.

[0081] Zeolite builders may suitably be present in a total amount offrom 5 to 60 wt %, preferably from 10 to 50 wt %.

[0082] The zeolites may be supplemented by other inorganic builders, forexample, amorphous aluminosilicates, or layered silicates such as SKS-6ex Clariant.

[0083] The zeolites may be supplemented by organic builders, forexample, polycarboxylate polymers such as polyacrylates andacrylic/maleic copolymers; monomeric polycarboxylates such as citrates,gluconates, oxydisuccinates, glycerol mono-, di- and trisuccinates,carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates,hydroxyethyliminodiacetates, alkyl- and alkenylmalonates and succinates;and sulphonated fatty acid salts.

[0084] Alternatively, the compositions of the invention may containphosphate builders, for example, sodium tripolyphosphate.

[0085] These lists of builders are not intended to be exhaustive.

[0086] Especially preferred organic builders are citrates, suitably usedin amounts of from 1 to 30 wt %, preferably from 2 to 15 wt %; andacrylic polymers, more especially acrylic/maleic copolymers, suitablyused in amounts of from 0.5 to 15 wt %, preferably from 1 to 10 wt %.Builders, both inorganic and organic, are preferably present in alkalimetal salt, especially sodium salt, form.

[0087] Detergent compositions according to the invention may alsosuitably contain a bleach system. Preferably this will include a peroxybleach compound, for example, an inorganic persalt or an organicperoxyacid, capable of yielding hydrogen peroxide in aqueous solution.

[0088] Preferred inorganic persalts are sodium perborate monohydrate andtetrahydrate, and sodium percarbonate, the latter being especiallypreferred. The sodium percarbonate may have a protective coating againstdestabilisation by moisture. The peroxy bleach compound is suitablypresent in an amount of from 5 to 35 wt %, preferably from 10 to 25 wt%. The peroxy bleach compound may be used in conjunction with a bleachactivator (bleach precursor) to improve bleaching action at low washtemperatures. The bleach precursor is suitably present in an amount offrom 1 to 8 wt %, preferably from 2 to 5 wt %. Preferred bleachprecursors are peroxycarboxylic acid precursors, more especiallyperacetic acid precursors and peroxybenzoic acid precursors; andperoxycarbonic acid precursors. An especially preferred bleach precursorsuitable for use in the present invention is N,N,N′,N′-tetracetylethylenediamine (TAED).

[0089] A bleach stabiliser (heavy metal sequestrant) may also bepresent. Suitable bleach stabilisers include ethylenediaminetetraacetate (EDTA), diethylenetriamine pentaacetate (DTPA),ethylenediamine disuccinate (EDDS), and the polyphosphonates such as theDequests (Trade Mark), ethylenediamine tetramethylene phosphonate(EDTMP) and diethylenetriamine pentamethylene phosphate (DETPMP).

[0090] The compositions of the invention may contain alkali metal,preferably sodium, carbonate, in order to increase detergency and easeprocessing. Sodium carbonate may suitably be present in amounts rangingfrom 1 to 60 wt %, preferably from 2 to 40 wt %. Sodium silicate mayalso be present, suitably in an amount of from 0.1 to 5 wt %.

[0091] Powder flow may be improved by the incorporation of a smallamount of a powder structurant. Examples of powder structurants, some ofwhich may play also other roles in the formulation, include, forexample, fatty acids (or fatty acid soaps), sugars, acrylate oracrylate/maleate polymers, sodium silicate, and dicarboxylic acids (forexample, Sokalan (Trade Mark) DCS ex BASF). One preferred powderstructurant is fatty acid soap, suitably present in an amount of from 1to 5 wt %.

[0092] Other materials that may be present in detergent compositions ofthe invention include antiredeposition agents such as cellulosicpolymers; soil release agents; anti-dye-transfer agents; fluorescers;inorganic salts such as sodium sulphate; enzymes (proteases, lipases,amylases, cellulases); dyes; colored speckles; perfumes; and fabricconditioning compounds. This list is not intended to be exhaustive.

Detergent Composition Product Form and Preparation

[0093] The detergent compositions of the invention are in particulateform. Particulate detergent compositions comprise powders, and tabletsof compacted powder. They may be prepared by any of the methods suitablefor the preparation of such compositions.

[0094] Powders of low to moderate bulk density may be prepared byspray-drying a slurry, and optionally postdosing (dry-mixing) furtheringredients. “Concentrated” or “compact” powders may be prepared bymixing and granulating processes, for example, using a high-speedmixer/granulator, or other non-tower processes.

EXAMPLES

[0095] The invention is illustrated in further detail by the followingnon-limiting Examples, in which parts and percentages are by weightunless otherwise stated.

[0096] The following parameters and test methods are used in theExamples.

Dynamic Flow Rate

[0097] Powder flow may be quantified by means of the dynamic flow rate(DFR), in ml/s, measured by means of the following procedure. Theapparatus used consists of a cylindrical glass tube having an internaldiameter of 35 mm and a length of 600 mm. The tube is securely clampedin a position such that its longitudinal axis is vertical. Its lower endis terminated by means of a smooth cone of polyvinyl chloride having aninternal angle of 15° and a lower outlet orifice of diameter 22.5 mm. Afirst beam sensor is positioned 150 mm above the outlet, and a secondbeam sensor is positioned 250 mm above the first sensor.

[0098] To determine the dynamic flow rate of a powder sample, the outletorifice is temporarily closed, for example, by covering with a piece ofcard, and powder is poured through a funnel into the top of the cylinderuntil the powder level is about 10 cm higher than the upper sensor; aspacer between the funnel and the tube ensures that filling is uniform.The outlet is then opened and the time t (seconds) taken for the powderlevel to fall from the upper sensor to the lower sensor is measuredelectronically. The measurement is normally repeated two or three timesand an average value taken. If V is the volume (ml) of the tube betweenthe upper and lower sensors, the dynamic flow rate DFR (ml/s) is givenby the following equation:${DFR} = {\frac{V}{t}\quad {ml}\text{/}s}$

[0099] The averaging and calculation are carried out electronically anda direct read-out of the DFR value obtained.

Compressibility

[0100] The method of measuring compressibility used in the presentinvention is as follows.

[0101] The experiment is carried out at 20-25° C. and a relativehumidity of about 40%. These values represent typical ambient conditionsin a northern European indoor laboratory environment. The exact relativehumidity at which the measurement is carried out is not critical,provided that it is not so high that the samples take up moisture.

[0102] The apparatus comprises a perspex cylinder with an internaldiameter of 54 mm and a height of 170 mm. The side of the cylinder isgraduated in millimeters. A piston is provided which fits the internaldiameter of the perspex cylinder.

[0103] The top of the piston has means to support a weight, wherebypressure can be applied to detergent powder contained in the perspexcylinder. The combined mass of the piston and the weight is 25 kg.

[0104] To measure the compressibility of a sample, the perspex cylinderis filled with particulate detergent composition (hereinafter “powder”).The top of the layer of powder is levelled by removing superfluouspowder with a straight-edge. Thus, a standard volume of powder istested. The initial volume is measured by means of the scale on the sideof the cylinder. The piston and weight are then lowered onto the surfaceof the powder and are allowed to rest freely on the powder for 60seconds. The volume of the powder after 60 seconds is measured by meansof the scale on the side of the cylinder.

[0105] The volume reduction is used to calculate the compressibilityusing the following equation:$\underset{({{in}\quad \%})}{Compressibility} = {\frac{\left( {{{initial}\quad {volume}} - {{final}\quad {volume}}} \right)}{{initial}\quad {volume}} \times 100}$

[0106] Components having a compressibility of 17% or more can lead tostickiness or storage problems if present at too high a level.

Example 1

[0107] A granular detergent component was prepared to the followingnominal formulation: Weight % Cationic surfactant 30.00 (as anhydrousmaterial) Sodium carbonate 68.00 Zeolite 2.00

[0108] The cationic surfactant was C₁₂-C₁₄ alkyl dimethyl hydroxyethylammonium chloride, Praepagen HY (Trade Mark), supplied by Clariant GmbHas a 40 wt % aqueous solution.

[0109] The granules were prepared in an approximately 10 kg batchprocess using a Vomatec (Trade Mark) fluidised bed. Starting materialsused were as follows: kg Cationic surfactant (40% solution) 11.4Anhydrous sodium carbonate (light soda ash) 10.0 Zeolite MAP powder 0.4

[0110] The light soda ash, which had a starting average particle size of90 micrometres, was fluidised using air at 120° C., and the cationicsurfactant solution, preheated to 600° C., was sprayed on. As thesolution encountered the sodium carbonate particles, the water wasrapidly driven off leaving the cationic surfactant deposited onto thesodium carbonate. Further deposition and evaporation took place, withsome agglomeration, until the granules within the fluid bed containedabout 30 wt % of cationic surfactant. The resulting granules were cooledusing fluidising air at ambient temperature (20° C.), and zeolite waslayered on.

[0111] The granules had the following properties: Measured cationicsurfactant content (wt %) 31.6 Bulk density (g/l) 588 Dynamic flow rate(ml/s) 134 Compressibility (vol %) 12.4 Average particle size d₅₀(micrometer) 394 Particles <180 micrometer (wt %) 2.5 Dissolution timeT₉₀ (s) 16 Loss at 135° C. (wt %) 1.6

Examples 2 TO 8

[0112] Example 1 was repeated using the solids mixes listed below toreplace the 10 kg light soda ash used in Example 1. Example 2 3 4 5 6 78 Ingredient (kg) Light soda ash 9 9 8 9 9 9 9 Na alk. silicate 1Calcite 1 2 (Durcal 15) 15 μm Calcite 1 (Durcal 40) 40 μm Kaolin 1Speswhite 1 clay (kaolin) STP 1 Zeolite MAP 0.4 0.4 0.4 0.4 0.4 0.4 0.4Measured cationic 29.2 31.0 30.9 29.4 29.3 26.2 23.8 surfactant content(wt %) Bulk density g/l 509 497 509 520 509 588 599 DFR (ml/s) 109 103113 110 104 99 64

Example 9

[0113] Granules to the nominal composition given in Example 1 wereprepared on a larger scale using a Niro fluid bed suitable for 100kgbatch operation. The cationic surfactant solution, preheated to 60° C.,was sprayed onto 75 kg of light soda ash in a 0.5 m² bed withfluidisation by air at 130° C. After the required amount of cationicsurfactant solution had been added, the granulated material was passedthrough the remainder of the fluid bed using air at ambient temperature(20°C.). The cooled granules were sieved and then layered with 2 wt %zeolite in a concrete mixer. The properties of the granules were asshown below. Measured cationic surfactant content (wt %) ca. 30 Bulkdensity (g/l) 700 Dynamic flow rate (ml/s) 140 Compressibility (vol %)10.0 Average particle size d₅₀ (micrometer) 500 Particles <180micrometer (wt %) <5 Dissolution time T₉₀ (s) <20 Loss at 135° C. (wt %)4.7

Example 10

[0114] A granular detergent component was prepared to the followingnominal formulation: Weight % Cationic surfactant 34.00 (as anhydrousmaterial) Zeolite MAP 58.00 Water 8.00

[0115] The cationic surfactant and zeolite MAP were as used in Example1.

[0116] The granules were prepared in an approximately 10 kg batchprocess using a Vomatec (Trade Mark) fluidised bed. Starting materialsused were as follows: kg Cationic surfactant (40% solution) 14.65Zeolite MAP 10.0

[0117] The zeolite MAP, which had a starting average particle size of 1micrometer, was fluidised using air at 120° C., and the cationicsurfactant solution, preheated to 60° C., was sprayed on. As thesolution encountered the zeolite particles, the water was rapidly drivenoff leaving the cationic surfactant deposited onto the zeolite. Furtherdeposition and evaporation took place, with some agglomeration, untilthe granules within the fluid bed contained about 34 wt % of cationicsurfactant. The resulting granules were cooled using fluidising air atambient temperature (20° C.), and zeolite was layered on.

[0118] The granules had the following properties: Measured cationicsurfactant content (wt %) ca. 34 Bulk density (g/l) 578 Dynamic flowrate (ml/s) 137 Compressibility (vol %) 8.0 Average particle size d₅₀(micrometer) 585 Particles <180 micrometer (wt %) <5 Dissolution timeT₉₀ (s) 84

Example 11

[0119] Granules to the nominal composition given in Example 10 wereprepared on a larger scale using a Hutlin fluid bed suitable for 500 kgbatch operation. The cationic surfactant solution, preheated to 60° C.,was sprayed onto 375 kg of light soda ash in a 1.5 m² bed withfluidisation by air at 130° C. After the required amount of cationicsurfactant solution had been added, the granulated material was passedthrough the remainder of the fluid bed using air at ambient temperature(20°C.). The cooled granules were sieved and then layered with 2 wt %zeolite in a concrete mixer. The properties of the granules were asshown below. Measured cationic surfactant content (wt %) ca. 34 Bulkdensity (g/l) 785 Dynamic flow rate (ml/s) 147 Compressibility (vol %)4.0 Average particle size d₅₀ (micrometer) 537 Particles <180 micrometer(wt %) <5 Dissolution time T₉₀ (s) 100

We claim:
 1. A process for the preparation of a granular detergentcomponent comprising (a) at least 20 wt % of a surfactant selected fromcationic surfactants, zwitterionic surfactants, amphoteric surfactantsand mixtures thereof, (b) an inorganic carrier material, which processcomprises spraying an aqueous solution of the surfactant (a) onto movinggranules of the inorganic carrier material (b) in the presence of adrying gas at a temperature within the range of from 65 to 200° C.
 2. Aprocess as claimed in claim 1, carried out at a temperature within therange of from 80 to 200° C.
 3. A process as claimed in claim 2, carriedout at a temperature within the range of from 100 to 150° C.
 4. Aprocess as claimed in claim 1, carried out in a fluidised bed.
 5. Aprocess as claimed in claim 1, carried out in a fluidised bed, whichcomprises the steps of (i) fluidising granules of the inorganic carriermaterial (b) using a gas having a temperature within the range of from100 to 150° C., (ii) spraying an aqueous solution of the surfactant (a)onto the mass of fluidised granules, (iii) cooling the resultinggranular detergent component by mixing in the presence of a gas having atemperature not exceeding 50° C.
 6. A process as claimed in claim 5,wherein the drying and cooling gases used in steps (i) and (iii) areair.
 7. A process as claimed in claim 5, wherein the aqueous solution ofthe surfactant (a) is preheated to a temperature within the range offrom 50 to 70° C.
 8. A process as claimed in claim 5, wherein thecooling step (iii) is carried out in a fluidised bed.
 9. A process asclaimed in claim 1, wherein the aqueous solution of the surfactant (a)has a concentration of less than 50 wt %, preferably from 30 to 45 wt %.10. A process as claimed in claim 1, wherein the aqueous solution of thesurfactant (a) is free of anionic surfactants.
 11. A process as claimedin claim 1, wherein the surfactant (a) comprises a cationic surfactantwhich is a water-soluble quaternary ammonium salt of the general formulaI R₁R₂R₃R₄N⁺X⁻  (I) wherein R₁ is a C₈-C₁₈ hydrocarbon group, optionallyinterrupted with a heteroatom or an ester or amide group; each of R₂, R₃and R₄ (which may be the same or different) is a C₁-C₃ alkyl orsubstituted alkyl group; and X is a solubilising anion.
 12. A process asclaimed in claim 11, wherein in the compound of the formula I R₁ is aC₈-C₁₈ alkyl group, more preferably a C₈-C₁₀ or C₁₂-C14 alkyl group, R₂is a methyl group, and R₃ and R₄, which may be the same or different,are methyl or hydroxyethyl groups.
 13. A process as claimed in claim 1,which further comprises the step of coating the granular detergentcomponent with an outer layer of finely divided water-insoluble flowaid, preferably selected from zeolites and amorphous aluminosilicates.14. A process as claimed in claim 1, wherein the granular detergentcomponent contains at least 25 wt %, preferably at least 30 wt %, of thesurfactant (a).
 15. A process as claimed in claim 1, which is carriedout as a batch process.
 16. A process as claimed in claim 1, whichincludes a preliminary step wherein a partial quantity of the surfactant(a) is added to the inorganic carrier material prior to spraying theaqueous solution of the surfactant (a) onto moving granules of theinorganic carrier material (b) in the presence of a drying gas.
 17. Aprocess as claimed in claim 16 where the preliminary step is apre-granulation step, carried out in a mixer/granulator.
 18. A processas claimed in claim 1, wherein at least 80 wt % of the inorganic carriermaterial is water-soluble.
 19. A process as claimed in claim 18, whereinthe inorganic carrier material comprises from 80 to 100 wt % of awater-soluble material selected from sodium carbonate, sodiumtripolyphosphate and mixtures thereof, and optionally up to 20 wt % of awater-insoluble material.
 20. A process as claimed in claim 19, whereinthe inorganic carrier material comprises from 80 to 100 wt % of sodiumcarbonate, and optionally up to 20 wt % of a water-insoluble inorganiccarrier material selected from aluminosilicates, silicas, clays andcalcite.
 21. A process as claimed in claim 1, wherein the granulardetergent component comprises from 20 to 40 wt % of the surfactant (a),and from 60 to 80 wt % of sodium carbonate.
 22. A process as claimed inclaim 1, wherein the inorganic carrier material comprises from 80 to100% of water-insoluble material.
 23. A process as claimed in claim 1,wherein the inorganic carrier material comprises crystalline alkalimetal aluminosilicate.
 24. A process as claimed in claim 23, wherein theinorganic carrier material comprises from 20 to 100% of crystallinealkali metal aluminosilicate.
 25. A process as claimed in claim 23,wherein the inorganic carrier material comprises from 80 to 100% ofcrystalline alkali metal aluminosilicate.
 26. A process as claimed inclaim 23, wherein the inorganic carrier material comprises a crystallinealkali metal aluminosilicate which is zeolite MAP.
 27. A process asclaimed in claim 23, which comprises from 20 to 40 wt % of thesurfactant (a), and from 60 to 80 wt % of crystalline alkali metalaluminosilicate.
 28. A granular detergent component which comprises (a)at least 20 wt % of a surfactant selected from cationic surfactants,zwitterionic surfactants, amphoteric surfactants and mixtures thereof,(b) an inorganic carrier material, the component being free from sodiumsulphate.
 29. A granular detergent component as claimed in claim 28,which comprises at least 30 wt % of the surfactant (a).
 30. A granulardetergent component as claimed in claim 28, which is free from anionicsurfactants.
 31. A granular detergent component as claimed in claim 28,where at least 80% of the inorganic carrier material (b) iswater-soluble.
 32. A granular detergent component as claimed in claim31, wherein at least 80 wt % of the inorganic carrier material comprisessodium carbonate, sodium tripolyphosphate or a mixture thereof.
 33. Agranular detergent component as claimed in claim 31, which comprisesfrom 20 to 40 wt % of the surfactant (a), and from 60 to 80 wt % ofsodium carbonate.
 34. A granular detergent component as claimed in claim28, wherein the inorganic carrier material comprises from 80 to 100% ofwater-insoluble material.
 35. A granular detergent component as claimedin claim 28, wherein the inorganic carrier material comprisescrystalline alkali metal aluminosilicate.
 36. A granular detergentcomponent as claimed in claim 35, wherein the inorganic carrier materialcomprises from 20 to 100% of crystalline alkali metal aluminosilicate.37. A granular detergent component as claimed in claim 35, wherein theinorganic carrier material comprises from 80 to 100% of crystallinealkali metal aluminosilicate.
 38. A granular detergent component asclaimed in claim 35, wherein the inorganic carrier material comprises acrystalline alkali metal aluminosilicate which is zeolite MAP.
 39. Agranular detergent component as claimed in claim 35, which comprisesfrom 20 to 40 wt % of the surfactant (a), and from 60 to 80 wt % ofcrystalline alkali metal aluminosilicate.
 40. A granular detergentcomponent as claimed in claim 28, which contains less than 5 wt % ofalkali metal silicate.
 41. A particulate laundry detergent compositioncomprising in total from 5 to 60 wt % of one or more organic detergentsurfactants, from 10 to 80 wt % of one or more detergency builders andoptionally other detergent ingredients, which composition includes agranular detergent component as claimed in claim 28.